Effect of Hydrochloric Acid Hydrolysis under Sonication and Hydrothermal Process to Produce Cellulose Nanocrystals from Oil Palm Empty Fruit Bunch (OPEFB)

This paper presents an approach for hydrolyzing cellulose nanocrystals from oil palm empty fruit bunch (OPEFB) presented through hydrochloric acid hydrolysis under sonication–hydrothermal conditions. Differences in concentration, reaction time, and acid-to-cellulose ratio affect toward the yield, crystallinity, microstructure, and thermal stability were obtained. The highest yield of cellulose nanocrystals up to 74.82%, crystallinity up to 78.59%, and a maximum degradation temperature (T_max) of 339.82 °C were achieved through hydrolysis using 3 M HCl at 110 °C during 1 h. X-ray diffraction analysis indicated a higher diffraction peak pattern at 2θ = 22.6° and a low diffraction peak pattern at 2θ = 18°. All cellulose nanocrystals showed a crystalline size of under 1 nm, and it was indicated that the sonication–hydrothermal process could reduce the crystalline size of cellulose. Infrared spectroscopy analysis showed that a deletion of lignin and hemicellulose was demonstrated in the spectrum. Cellulose nanocrystal morphology showed a more compact structure and well-ordered surface arrangement than cellulose. Cellulose nanocrystals also had good thermal stability, as a high maximum degradation temperature was indicated, where CNC-D1 began degrading at temperatures (T₀) of 307.09 °C and decomposed (T_max) at 340.56 °C.